CN105585861B - A kind of modified pitch particle and preparation method thereof - Google Patents
A kind of modified pitch particle and preparation method thereof Download PDFInfo
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- CN105585861B CN105585861B CN201410564711.1A CN201410564711A CN105585861B CN 105585861 B CN105585861 B CN 105585861B CN 201410564711 A CN201410564711 A CN 201410564711A CN 105585861 B CN105585861 B CN 105585861B
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Abstract
The invention discloses a kind of modified pitch particle and preparation method thereof, based on modified pitch particle weight part, including following component：15~60 parts of high softening point bitumen I；10 ~ 50 parts of high softening point bitumen II；20~50 parts of rubber powder granule；Described high softening point bitumen II is wrapped in outside rubber powder granule, and high softening point bitumen I is wrapped in outside high softening point bitumen II；Wherein high softening point bitumen II and high softening point bitumen I softening point difference is 10 ~ 25 DEG C.Modified pitch particle of the present invention has higher softening point, and high-temperature behavior is excellent, and preparation method is simple, can persistently be played a role under the conditions of the drillng operation of wide temperature range in deep layer drilling well, plays good closure and filtrate reducing effect.
Description
Technical field
The invention belongs to asphalt field, and in particular to a kind of modified pitch particle and preparation method thereof.
Background technology
Asphalt product is one of important additive for drilling fluid, with good anti-collapse, lubrication, emulsification, filtrate reducing and height
The comprehensive effectivenesses such as temperature stabilization.Asphalt product typically contains water insoluble pitch particle, and has certain softening point.Work as well
When intraocular has sufficiently high temperature and pressure, pitch particle softening transform, and being squeezed into borehole wall microcrack, prevent drilling fluid and
Filtrate is permeated from microcrack, and stratum is effectively blocked together with mud cake.Bitumen is that oil drilling is extremely effective anti-collapse
Agent and oil layer protective agent.With the development of Petroleum finance, drilling depth is constantly deepened, and drilling strata is more and more complicated,
The quantity of the special wells such as directional well, horizontal well gradually increases.This make drilling engineering to drilling fluid asphalt product and its
System proposes higher requirement.The high softening point bitumen that high-temperature behavior is good, have good seal-off effect and filtration reduction is developed (to refer to
Softening point is more than 100 DEG C, especially more than 120 DEG C), the need for meeting oil drilling engineering, with highly important
Meaning.
The preparation technology of high softening point bitumen typically use solvent deasphalting or air blowing oxidation technique, CN102464989A,
CN102876344A, CN102464988A and CN102382696A etc. disclose several high softening point bitumens being used in drilling fluid
Or the preparation method of pitch particle, asphalt softening point is typically more than 120 DEG C, up to 250 DEG C.
CN102952526A discloses a kind of high softening-point emulsified asphalt water-base drilling fluid inorganic agent and preparation method thereof, institute
State additive for drilling fluid including 40~70% softening points for 150~240 DEG C pitch, 35~50 weight % water, 0.02~2% auxiliary agent,
0.05~5 % emulsifying agents, 0.01~1% stabilizer, additive for drilling fluid has good HTHP filtrate reducing function, fits
Deep-well and ultra-deep well drilling for HTHP.
US7220348B1, CN102876344 A, CN102876344 A and CN102732280A also disclose several high soft
Change the production method of point pitch, asphaltic products softening point is all at 250 DEG C with but mainly for the production of carbon fiber product, fire proofed wood
Expect binding agent and spinning field.
It is single due to constituting when existing high softening point bitumen is among applied to drilling fluid system, there is viscoelastic scope
It is smaller, the problems such as temperature in use scope is narrower, it is difficult to persistently be played a role in underground.CN1046176A discloses a kind of containing pre-
About 2 parts of high softening-point pitch of mixing, about 1 part of low softening point pitch, about 1 part of causticization lignite and a kind of strongly lipophilic are non-
The water-based drilling muds additive of ionic surface active agent.This compositions of additives can be in the temperature and pressure of wide scope
Effectively, but simple mechanical mixture is difficult the effective action effect for playing different softening point pitch.Using several different softenings
Point pitch mechanical mixture, simple combination is also all each to play a role, after softening point, just ineffective, it is desirable to not
Good plugging effect is reached in synthermal scope to ensure the addition of every kind of softening point asphalt, further increases drip
The blue or green difficulty disperseed in drilling fluid.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of modified pitch particle and preparation method thereof.The present invention is modified
Pitch particle has higher softening point, and high-temperature behavior is excellent, with good deformability, and preparation method is simple, in deep layer
It can persistently be played a role under the conditions of the drillng operation of wide temperature range during drilling well, play good closure and filtrate reducing effect
Really.
The modified pitch particle of the present invention, by weight, including following component：
15~60 parts of high softening point bitumen I；
10 ~ 50 parts of high softening point bitumen II；
20~50 parts of rubber powder granule；
Described high softening point bitumen I is wrapped in outside rubber powder granule, and high softening point bitumen II is wrapped in high softening-point drip
Outside blue or green I；Wherein high softening point bitumen II and high softening point bitumen I softening point difference is 10 ~ 25 DEG C.
Described high softening point bitumen I softening point is 150 ~ 280 DEG C, preferably 180 ~ 260 DEG C；Wherein high softening point bitumen
I can be commercially available prod or natural pitch, can also be prepared according to this area routine techniques, such as reduced pressure distillation process, solvent
De-asphalting processes, air blowing oxidation technique etc., or several techniques combination.
Described high softening point bitumen II softening point is 160~300 DEG C, preferably 180~280 DEG C；High softening-point is dripped
Blue or green II can be commercially available prod or natural pitch, can also be prepared according to this area routine techniques, such as reduced pressure distillation process, molten
Agent de-asphalting processes, air blowing oxidation technique etc., or several techniques combination.
Described rubber powder can be prepared for commercially available waste-tyre rubber-powder product or according to existing method, and particle diameter is 60 ~ 250
Mesh, preferably 80 ~ 200 mesh.
The average grain diameter of the modified pitch particle of the present invention is less than 60 mesh.
Accelerator is preferably added in the modified pitch particle of the present invention, on the basis of modified pitch particle weight, accelerator
Addition is 1wt%~10wt%, and wherein accelerator is the one or more in sulfate, quaternary ammonium salt or lignosulfonates, its
Middle sulfate is the one or more in modified bay alcohol radical sodium sulphate, secondary alcohol groups sodium sulphate and mixed fatty alcohol sodium sulphate etc.；
Quaternary ammonium salt is in DTAC, hexadecyltrimethylammonium chloride, OTAC etc.
It is one or more of；Lignosulfonates are sodium lignin sulfonate or calcium lignosulfonate.
The preparation method of the modified pitch particle of the present invention, including following content：
（1）High softening point bitumen I and compatilizer are mixed to get mother liquor I, mother liquor I is uniformly then sprayed onto rubber powder
On grain, permeated by standing, compatilizer is then removed under vacuumized conditions, leftover materials are chilled, crush, obtained modification
Rubber powder granule.
（2）High softening point bitumen II and compatilizer are mixed to get mother liquor II, then by step（1）Obtained modified glue powder
Particle is well mixed in the reactor with mother liquor II, and being passed through compressed gas from reactor bottom carries out stripping processing, and compatilizer is in
The reacted device upper outlet discharge of gas phase, can be recycled through cooling, and after stripping terminates, discharging, cooling obtains high softening-point drip
Blue or green mixture；
（3）By step（2）Obtained mixture, surfactant and inorganic micro powder, which is added in disintegrating apparatus, to be mixed
Crush, prepare modified pitch particle.
In the inventive method, step（1）With（2）Described compatilizer is that boiling range scope is any between 100 ~ 350 DEG C
One or more in cut, any cut between preferably 150 ~ 300 DEG C, such as gasoline, kerosene or diesel oil.
In the inventive method, step（1）The mass ratio that described compatilizer is mixed with high softening point bitumen I is 1:5~2:1,
It is preferred that 1:3~1:1.
In the inventive method, step（1）Described high softening point bitumen I is 20 ~ 80 DEG C with compatilizer mixing temperature, preferably
25~75℃.Incorporation time is 5 ~ 60 minutes, and preferably 10 ~ 30 minutes, mixed process can be using common churned mechanically side
Formula, is well mixed the two.
In the inventive method, step（1）Described sprinkling process can use with spraying function equipment, such as watering can,
Spraying machine, sprayer etc., can be stirred or be mixed and stirred to material during sprinkling, mother liquor I is dispersed in rubber powder
Grain surface.
In the inventive method, step（1）Described standing time of penetration is 0.5 ~ 5 hour.
In the inventive method, step（1）Described vacuumized conditions are：30 ~ 130 DEG C of temperature, preferably 55 ~ 100 DEG C, pressure
Power≤8kPa, the time is 0.5 ~ 5 hour, preferably 1 ~ 3 hour.
In the inventive method, step（1）The condition of described freezing is：Cryogenic temperature be -10~-50 DEG C, preferably -20 ~ -
40 DEG C, preferably cooling time 5~24 hours, 10 ~ 18 hours.Vibration grinding time is 1~100s, preferably 10~50s
In the inventive method, step（1）Obtained modified glue powder particle is preferably dry-mixed with inorganic micro powder progress, wherein pitch
Mass ratio with inorganic micro powder is 10：1~100：1, described inorganic micro powder is in graphite, montmorillonite, bentonite or hydrotalcite
One or more, the granularity of inorganic micro powder is less than 100 μm, preferably nano grade inorganic micro mist, and above-mentioned inorganic micro powder is preferably through having
The inorganic micro powder that machine is modified, such as silane coupler, titanate coupling agent organic modifiers.
In the inventive method, step（2）The mass ratio that described compatilizer is mixed with high softening point bitumen II is 1:4~2:
1, preferably 1:3~1:1.
In the inventive method, step（2）Described compressed gas is one kind or several in air, nitrogen or inert gas
Kind.
In the inventive method, step（2）Described high softening point bitumen II is 20 ~ 80 DEG C with compatilizer mixing temperature, excellent
Select 25 ~ 75 DEG C.Incorporation time is 5 ~ 60 minutes, and preferably 10 ~ 30 minutes, mixed process can be using common churned mechanically side
Formula, is well mixed the two.
In the inventive method, step（2）Described reactor is the reaction vessel with agitating function, and reactor lower part is set
There is compressed gas entrance, top is provided with gas vent.
The condition of described stripping processing is：120~300 DEG C of stripping temperature, preferably 160~280 DEG C, stripping time is
0.3~3 hour, compressed gas inlet pressure was 0.1 ~ 0.5MPa.
Stripping processing procedure is preferably carried out as follows：In 120 ~ 250 DEG C of temperature, carry out stripping and handle 20 ~ 150 points
Clock, then heats to 140 ~ 300 DEG C, stripping 10 ~ 100 minutes.Described stripping temperature is consistently less than high softening point bitumen II's
Softening point.
In the inventive method, step（3）Described surfactant is DTAC, cetyl three
One or more in ammonio methacrylate, OTAC, sodium lignin sulfonate or calcium lignosulfonate etc., plus
Enter amount accounts for high softening point bitumen particle weight 0.05% ~ 5%, preferably 0.5% ~ 3%.
In the inventive method, step（3）Described inorganic micro powder is one in graphite, montmorillonite, bentonite or hydrotalcite
Kind or it is several, the granularity of inorganic micro powder is less than 100 μm, preferably nano grade inorganic micro mist, and above-mentioned inorganic micro powder is preferably through organic
Modified inorganic micro powder, addition accounts for the 1% ~ 10% of high softening point bitumen particle weight, preferably 3% ~ 5%.
In the inventive method, described disintegrating apparatus can be high energy shear milling machine, colloid mill, ball mill pulverizer, shake
The disintegrating apparatus such as dynamic sieve, grinding time is 10~60s, and it is no more than 30 DEG C to crush temperature, and high softening point bitumen is preferably being crushed
Preceding to carry out low temperature brittleness processing, low temperature brittleness treatment conditions are：Temperature is 0~-60 DEG C, is preferably -10~-30 DEG C, the time is 2
~48 hours, preferably 2~10 hours.
In the inventive method, phosphate shallow lake can also be added in the preparation process of described modified pitch particle as needed
One in powder, CMS, cationic starch, carboxymethyl cellulose (CMC), vinal and WATER-SOLUBLE PVA FIBER
Plant or several.
The modified pitch particle of the present invention is in terms of oil drilling, the particularly deep layer wellbore fluid of wide temperature
Applied in system.
Compared with the high low softening point asphalt of direct mechanical mixture in the prior art, the advantage of the invention is that：
（1）The modified pitch particle of the present invention has the structure of " outer layer-intermediate layer-nuclear phase ", and outer layer asphalt softening point is high
In 10 ~ 25 DEG C of the softening point of intermediate layer pitch, well temperature two kinds of softening points it is interval and near change when, intermediate layer mutually first softens,
But due to the presence of outer layer pitch and nuclear phase rubber powder granule, it will not trickle, when being extruded by external force, pitch particle is easy
Deformation, intermediate layer, outer layer and rubber powder granule viscoelastic sex differernce are also beneficial to be formed the mud cake of densification, play plugging action, widen
The Applicable temperature scope of high softening point bitumen composition grain.
（2）The crack or duct of oil-gas Layer are not of uniform size, and the deformability of simple high softening point bitumen particle is after all
It is limited, it is impossible to good match therewith, therefore easily cause duct of all size and shapes that can not be arbitrarily embedded into well etc. and ask
Topic, it is difficult to play preferably closure and filtrate reducing effect；The modified pitch particle of the present invention can centering according to the actual needs
The pitch of interbed phase and outer layer carries out the modulation of softening point, can persistently be played a role in the range of wider drilling depth, together
Shi Caiyong adds its viscoelastic using the rubber powder of suitable particle diameter as nuclear phase, that is, and uses scope, can be in wider pore-size distribution model
Enclose it is interior use, serve good closure and the effect of stabilizing borehole.High softening point bitumen particle of the present invention compared to single or
The high softening point bitumen of mechanical mixture, with stronger deformability, granular size can be adjusted according to actual needs, so that
With the closure in different size of hole in oil reservoir, good plugging effect is played.
Embodiment
The present invention will be further described by embodiment below, but it is not thereby limiting the invention, it is therein
Percentage composition is weight/mass percentage composition.The method of testing of softening point is carried out according to GB/T4507 methods.High temperature and high pre ssure filtration is pressed
SY/T5621 methods are determined.
Embodiment 1
（1）By high softening point bitumen I（Softening point is 180 DEG C）Mother liquor I is mixed to get with kerosene（Mixing quality ratio is 2:
1）, mother liquor I is uniformly then sprayed onto rubber powder granule（Mother liquor is 1 with rubber powder granule mass ratio:1）On, it is small by standing infiltration 2
When, then under vacuumized conditions（80 DEG C of temperature, pressure≤8kPa, time 2 h）Compatilizer is removed, leftover materials are chilled
（- 35 DEG C of cryogenic temperature, cooling time is 12 hours）, crush, obtained modified glue powder particle.
（2）Take 100g high softening point bitumens II（Softening point is 200 DEG C）It is placed in 70g boiling ranges for 150 ~ 170 DEG C of cut
In container, room temperature（25℃）Stirring 30 minutes, mother liquor II is made after being sufficiently mixed uniformly；By 60g modified glue powders particle and mother
Liquid II is mixed in the reactor, and is passed through compressed air, and gas inlet pressure is 0.15 MPa, and temperature of reactor is maintained at 180 ~
190 DEG C, stir 100 minutes, discharging, cooling obtains high softening point bitumen mixture；
（3）The high softening point bitumen mixture that 100g low temperature brittleness is handled（Low temperature brittleness condition：- 25 DEG C of temperature, time
8 hours）, 4g hydrotalcites and 1.5g sodium lignin sulfonates it is well mixed, be put into vibratory sieve, 80 mesh standard sieves, vibration are selected in sieve bottom
Crush and obtain modified pitch particle under 20s, sieve, be designated as A1.
Embodiment 2
（1）By high softening point bitumen I（Softening point is 220 DEG C）Mother liquor I is mixed to get with diesel oil（Mixing quality ratio is 1:
1）, then mother liquor I is uniformly sprayed onto on rubber powder particles（Mother liquor is 2 with rubber powder granule mass ratio：1）, by standing infiltration 3
Hour, then under vacuumized conditions（100 DEG C of temperature, pressure≤8kPa, 1 hour time）Remove compatilizer, leftover materials warp
Freezing（- 25 DEG C of cryogenic temperature, cooling time is 10 hours）, crush, obtained modified glue powder particle.
（2）Take 100g high softening point bitumens II（Softening point is 250 DEG C）It is placed in 50g diesel oil in container, 50 DEG C of room temperature is stirred
Mix 30 minutes, mother liquor II is made after being sufficiently mixed uniformly；100g modified glue powders particle is mixed in the reactor with mother liquor II,
And compressed air is passed through, gas inlet pressure is 0.25 MPa, and temperature of reactor is kept for 230 ~ 240 DEG C, is stirred 70 minutes, is gone out
Material, cooling obtains high softening point bitumen mixture；
（3）By high softening point bitumen compositions of the 100g through low temperature brittleness（Brittle treatment conditions be the same as Example 1）, 5g stones
Ink, 1g cetyl trimethylammonium bromides and 3g CMSs are well mixed, are put into vibratory sieve, and sieve bottom is accurate from 100 targets
Sieve, vibration is crushed and obtains modified pitch particle under 20s, sieve.
Embodiment 3
（1）By high softening point bitumen I（Softening point is 170 DEG C）Mother liquor I is mixed to get with gasoline（Mixing quality ratio is 3:
1）, then mother liquor I is uniformly sprayed onto on rubber powder particles（Mother liquor is 3 with rubber powder granule mass ratio:1）, by standing infiltration 1
Hour, then under vacuumized conditions（Temperature 50 C, pressure≤8kPa, 1.5 hours time）Remove compatilizer, leftover materials warp
Freezing（- 30 DEG C of cryogenic temperature, cooling time is 8 hours）, crush, obtained modified glue powder particle.
（2）Take 100g high softening point bitumens II（Softening point is 140 DEG C）It is placed in 100g gasoline in container, 80 DEG C of room temperature is stirred
Mix 35 minutes, mother liquor II is made after being sufficiently mixed uniformly；120g modified glue powders particle is mixed in the reactor with mother liquor II,
And it is passed through compressed air, gas inlet pressure is 0.3 MPa, and temperature of reactor is maintained at 150 ~ 160 DEG C, stirs 60 minutes, so
After be warming up to 165 DEG C, stir 10 minutes, discharging, cooling obtains high softening point bitumen mixture；
（3）100g bituminous compositions, 6g montmorillonites and 0.5g Cetyltrimethylammonium bromides are well mixed, is put into and shakes
120 mesh standard sieves are selected at dynamic sieve, sieve bottom, and vibration is crushed and obtains modified pitch particle under 25s, sieve.
Comparative example 1
100g high softening point bitumens I（Softening point is 180 DEG C）, 4g hydrotalcites and 1.5g sodium lignin sulfonates, be put into vibration
80 mesh standard sieves are selected at sieve, sieve bottom, and vibration is crushed and obtains high softening point bitumen particle under 20s, sieve, is designated as A4.
Comparative example 2
100g high softening point bitumens II（Softening point is 220 DEG C）, 5 graphite, 1g cetyl trimethylammonium bromides and 3g carboxylics
Methyl starch is well mixed, and is put into vibratory sieve, and 100 mesh standard sieves are selected at sieve bottom, and vibration is crushed and obtains pitch particle under 20s, sieve,
It is designated as A5.
Comparative example 3
High softening point bitumen I and high softening point bitumen II raw material and usage ratio be the same as Example 3, the drip of 100g high softening-points
Blue or green I and high softening point bitumen II mixture, 6g montmorillonites and 0.5g Cetyltrimethylammonium bromides, is put into vibratory sieve, sieve
120 mesh standard sieves are selected at bottom, and vibration is crushed and obtains pitch particle under 25s, sieve, is designated as A6.
The blue or green particle of A1 ~ A6 high softening-points is added to the base slurry prepared, high softening point bitumen particle loads account for base slurry
The 2% of weight, the filter loss after determining different temperatures aging respectively under the conditions of test pressure 3.45MPa, concrete outcome is shown in Table 1.
Wherein base slurry preparation method is as follows：The drip of 2.75g natrium carbonicum calcinatums is added in 1000mL water, 60g calcium bentonites, high-speed stirring is added
Mix 20 minutes and conserve 24 hours at room temperature, obtain 6% fresh water-based slurry.
Filter loss after the modified pitch particle different temperatures aging of table 1.
Note：Temperature is Aging Temperature in table, and digestion time is 16 hours.
Claims (29)
1. a kind of modified pitch particle, it is characterised in that：Based on modified pitch particle weight part, including following component：Height softening
15~60 parts of point pitch I；II 10 ~ 50 parts of high softening point bitumen；20~50 parts of rubber powder granule；Described high softening point bitumen I
It is wrapped in outside rubber powder granule, high softening point bitumen II is wrapped in outside high softening point bitumen I；Wherein high softening point bitumen II compares
High softening point bitumen I softening point is high 10 ~ 25 DEG C.
2. according to the modified pitch particle described in claim 1, it is characterised in that：Described high softening point bitumen I softening point
For 150~280 DEG C.
3. according to the modified pitch particle described in claim 1, it is characterised in that：Described high softening point bitumen I softening point
For 180~260 DEG C.
4. according to the modified pitch particle described in claim 1, it is characterised in that：The softening point of described high softening point bitumen II
For 160 ~ 300 DEG C.
5. according to the modified pitch particle described in claim 1, it is characterised in that：The softening point of described high softening point bitumen II
180~280℃。
6. according to the modified pitch particle described in claim 1, it is characterised in that：Described rubber powder is commercially available waste and old tyre rubber
Powder product is prepared according to existing method, and particle diameter is 60 ~ 250 mesh.
7. according to the modified pitch particle described in claim 1, it is characterised in that：The average grain diameter of modified pitch particle be less than
60 mesh.
8. according to the modified pitch particle described in claim 1, it is characterised in that：Accelerator is added in modified pitch particle, with
On the basis of modified pitch particle weight, accelerator addition be 1wt%~10wt%, wherein accelerator be sulfate, quaternary ammonium salt or
One or more in lignosulfonates；Wherein sulfate is modified bay alcohol radical sodium sulphate, secondary alcohol groups sodium sulphate and mixing
One or more in sodium alkyl sulfate；Quaternary ammonium salt be DTAC, hexadecyltrimethylammonium chloride,
One or more in OTAC；Lignosulfonates are sodium lignin sulfonate or calcium lignosulfonate.
9. a kind of preparation method of the modified pitch particle described in claim 1 ~ 8 any claim, it is characterised in that including
Following content：（1）High softening point bitumen I and compatilizer are mixed to get mother liquor I, mother liquor I is uniformly then sprayed onto rubber powder
On particle, permeated by standing, compatilizer is then removed under vacuumized conditions, leftover materials are chilled, crush, and what is obtained changes
Property rubber powder granule；
（2）High softening point bitumen II and compatilizer are mixed to get mother liquor II, then by step（1）Obtained modified glue powder particle
It is well mixed in the reactor with mother liquor II, being passed through compressed gas from reactor bottom carries out stripping processing, and compatilizer is in gas phase
Reacted device upper outlet discharge, can be recycled through cooling, after stripping terminates, and discharging, cooling obtains high softening point bitumen and mixed
Compound；（3）By step（2）Obtained mixture, surfactant and inorganic micro powder, which is added in disintegrating apparatus, carries out mixed powder
It is broken, that is, prepare modified pitch particle.
10. in accordance with the method for claim 9, it is characterised in that：Step（1）With（2）Described compatilizer is boiling range scope
Any cut between 100 ~ 350 DEG C.
11. in accordance with the method for claim 9, it is characterised in that：Step（1）With（2）Described compatilizer is boiling range scope
Any cut between 150 ~ 300 DEG C.
12. in accordance with the method for claim 9, it is characterised in that：Step（1）Described compatilizer and high softening point bitumen I
The mass ratio of mixing is 1:5~2:1.
13. in accordance with the method for claim 9, it is characterised in that：Step（1）Described high softening point bitumen I and compatilizer
Mixing temperature is 20 ~ 80 DEG C, and incorporation time is 5 ~ 60 minutes.
14. in accordance with the method for claim 9, it is characterised in that：Step（1）Described sprinkling process, which is used, has sprinkling work(
The equipment of energy, is stirred or is mixed and stirred to material during sprinkling, mother liquor I is dispersed in rubber powder particle surface.
15. in accordance with the method for claim 9, it is characterised in that：Step（1）Described standing time of penetration is 0.5 ~ 5 small
When.
16. in accordance with the method for claim 9, it is characterised in that：Step（1）Described vacuumized conditions are：Temperature 30 ~
130 DEG C, pressure≤8kPa, the time is 0.5 ~ 5 hour.
17. in accordance with the method for claim 9, it is characterised in that：Step（1）The condition of described freezing is：Cryogenic temperature
For -10~-50 DEG C, cooling time 5~24 hours.
18. in accordance with the method for claim 9, it is characterised in that：Step（2）Described compatilizer and high softening point bitumen II
The mass ratio of mixing is 1:4~2:1.
19. in accordance with the method for claim 9, it is characterised in that：Step（2）Described compressed gas be air, nitrogen or
One or more in inert gas.
20. in accordance with the method for claim 9, it is characterised in that：Step（2）Described high softening point bitumen II and compatilizer
Mixing temperature is 20 ~ 80 DEG C, and incorporation time is 5 ~ 60 minutes.
21. in accordance with the method for claim 9, it is characterised in that：Step（2）Described reactor is with agitating function
Reaction vessel, reactor lower part is provided with compressed gas entrance, and top is provided with gas vent.
22. in accordance with the method for claim 9, it is characterised in that：The condition of described stripping processing is：Stripping temperature 120
~300 DEG C, stripping time is 0.3~3 hour, and compressed gas inlet pressure is 0.1 ~ 0.5MPa；Described stripping temperature is all the time
Less than the softening point of high softening point bitumen II.
23. in accordance with the method for claim 22, it is characterised in that：Stripping processing procedure is carried out as follows：In temperature
120 ~ 250 DEG C of degree, carries out stripping and handles 20 ~ 150 minutes, then heat to 140 ~ 300 DEG C, stripping 10 ~ 100 minutes.
24. in accordance with the method for claim 9, it is characterised in that：Step（3）Described surfactant is dodecyl three
Ammonio methacrylate, hexadecyltrimethylammonium chloride, OTAC, sodium lignin sulfonate or lignin sulfonic acid
One or more in calcium.
25. in accordance with the method for claim 9, it is characterised in that：Step（3）Described inorganic micro powder be graphite, montmorillonite,
One or more in bentonite or hydrotalcite, the granularity of inorganic micro powder is less than 100 μm.
26. in accordance with the method for claim 9, it is characterised in that：Described disintegrating apparatus is high energy shear milling machine, colloid
One or more in mill, ball mill pulverizer or vibratory sieve, grinding time is 10~60s, and it is no more than 30 DEG C to crush temperature.
27. in accordance with the method for claim 9, it is characterised in that：Added in the preparation process of described modified pitch particle
One or more in phosphate ester starch, CMS, cationic starch, carboxymethyl cellulose and WATER-SOLUBLE PVA FIBER.
28. in accordance with the method for claim 9, it is characterised in that：The average grain diameter of modified pitch particle is less than 60 mesh.
29. application of the modified pitch particle in oil drilling described in claim 1 ~ 8.
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| CN105585862B (en) * | 2014-10-22 | 2017-11-24 | 中国石油化工股份有限公司 | A kind of modified asphalt composite particle and preparation method thereof |
| CN111117228B (en) * | 2019-12-31 | 2023-03-10 | 湖南华曙新材料科技有限责任公司 | Preparation method of high polymer powder material for optical fiber laser sintering |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1087061C (en) * | 1998-08-13 | 2002-07-03 | 王玉明 | Bidirectional rotation double-row double-blade spiral groove face sealing |
| CN102070909B (en) * | 2010-12-08 | 2013-01-09 | 中国石油集团西部钻探工程有限公司 | Cation modified asphalt and preparation method thereof |
| CN103804926B (en) * | 2012-11-07 | 2016-03-30 | 中国石油化工股份有限公司 | A kind of Asphalt composition particle and preparation method thereof |
| CN105585862B (en) * | 2014-10-22 | 2017-11-24 | 中国石油化工股份有限公司 | A kind of modified asphalt composite particle and preparation method thereof |
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